Compound lubricants



Patented Apr. 20, 1948 COMPOUND LUBRICANTS John M. Mulseiman,

to The Standard Oil .a corporation of Ohio 8 ti: Euclid, anigno gimp-m,ciev elz'nd, Ohiof No Drawing. Application October 14 1941,

Serial No. 414,071

1 17 Claims.

In the preparation or metal compounds of the reaction product 01. asulphide of phosphorus on a wax or sterol ester, I have found that thefinal products fall into two classes, in accordance with the particularmetal, the properties and characteristics being of two difierent orders;and combinations of the two groups are of particular utility, providingcombinations of properties not realized with compounds of one metal.

To the accomplishment of the foregoing and related ends, the invention,then, comprises the features hereinafter fully described, andparticularly pointed out in the claims, the following descriptionsetting forth in detail certain illustrative embodiments oi. theinvention, these being indicative however, of but a few of the variousways in which the principle of the invention may be employed.

The invention will be best understood by reference to an illustrativeexample: Phosphorus pentasulphide in amount of about 20 per cent isheated with neutral degras at approximately 300 F. for an hour. Afterseparation of sludge, which is largely phosphorus pentoxide, theproduct, substantially free of phosphorus is reacted with about 5 percent of arsenic trioxide and about 5 per cent of calcium oxide at atemperature of about 250 F. for an hour. After all constituents arecombined, the product is clear. This product may be employed per se inextreme pressure gear usages etc., or it can be mixed with oils,combinations with heavy steam refined lubricating stock for instancegiving particularly good results. In general, the amount of the metalcompound may be 0.01 to 100 per cent in various usages.

The metals employed in the reaction may be applied in the form 01'oxides or other convenient reactive compounds, and as indicated above,there are two separate groups or categories. The compounds formed frommetals below iron or copper in the E. M, E. series, as for examplearsenic, antimony, bismuth, chromium, mercury, silver, etc., giveproducts which are particularly protective against attack on metals towhich the lubricant is applied, and they are also strikingly resistantagainst break-down of an oil with which they are incorporated. They maybe regarded as antioxidants, using the term in a broad sense, withoutrestricted implication that merely oxygen is the cause of break-down.The other metal compounds, viz. those of metals not exceeding fourelectron orbits in groups I, II and III of the periodic system, as forinstance calcium, sodium, potassium, aluminum, zinc, beryllium,magnesium, etc, as well as barium, give products which particularly havea detergent action or cleaning action on metal surfaces. Furtherillustrative advantageous combinations are antimony and aluminum,arsenic and barium, antimony and barium, chromium and calcium, chromiumand barium, etc.

Instead of simultaneously reacting both metals with the reaction productof phosphorus sulphide and wax, th respective metals may be separatelyreacted with the reaction product of phosphorus sulphide and wax and theproducts may then be mixed. Equal portions may be employed, or dependingupon the particular usages in view the proportions may be high foreither the one type of metal compound or the other, as desired. Themetal compounds may be applied without oil admixture, as in extremepressure gear usages, or they may be mixed with oils, in desiredamounts; and in general the amounts of the metal compounds may be 0.01to per cent, according to the usages.

As the wax raw material, aside from degras, other waxes, as lanolin,carnauba, Japan wax, sperm oil, etc., may be employed, the normallynon-liquid waxes being particularly advantageous. The sulphide oiphosphorus may be pentasulphide, sesquisulphide, etc., and as indicatedthe reaction is efiected with heat, usually around 300 F., or somewhathigher or lower in some cases, and generally about an hour is required.The second reaction or conversion into the metal compounds also requiresheat, as for instance 200 to 300 F., and usually for about an hour.

Other modes of applying the principle of the invention may be employed,change being made as regards the details described, provided the fea.tures stated in any of the following claims or the equivalent of such,be employed.

I therefore particularly point out and distinctly -.claim as myinvention:

1. Compounds oi a heavy metal selected from the group consisting ofchromium and metals below iron in the E. M. F. series and of a metalselected from the group consisting of barium and metals having notmore-than tour electron orbits 3 selected from groups I, II and III oithe periodic system, and the reaction product a sulphide oi phosphorusand an oxygen-containing wax reacted at a temperature to separate aphosphorus and omen-containing residue.

2. A lubricant comprising a lubricating all containing an additive in anamount to improve the stability of the oil under conditions or usage,said additive comprising compounds of a heavy metal selected from thegroup consisting of chromium and metals below iron in the E. M. F.series and or a metal selected from the group consisting of barium andmetals having not more than four electron orbits selected from groups I,II and III of the periodic system, and the reaction product ofphosphorus pentasulphide and an oxygencontaining wax reacted at atemperature to separate a phosphorus and oxygen-containing residue.

3. Compounds of arsenic and of calcium and the reaction product of a.sulphide of phosphorus and an oxygen-containing wax reacted at atemperature to separate a phosphorus and oxygencontaining residue.

4. Compounds of antimony and of barium, and the reaction product or asulphide of phosphorus and an oxygen-containing wax reacted at atemperature to separate a phosphorus and oxygen-containing residue.

5. Compounds of chromium and of barium. and the reaction product of a.sulphide oi, phosphorus and an oxygen-containing wax reacted at atemperature to separate a phosphorus and oxygen containing residue.

6. Compounds of a heavy metal selected from the group consisting ofchromium and metals below iron in the E. M. F. series and of a metalselected from the group consisting of barium and metals having not morethan four electron orbits selected from groups I, II and III of theperiodic system, and the reaction product oi a sulphide of phosphorusand degras reacted at a, temperature to separate a phosphorus andoxygen-containing residue.

'7. A lubricant comprising a lubricating oil containing an additive inan amount to improve the stability of the oil under conditions of usage,said additive comprising compounds of a heavy metal selected from thegroup consisting of chromium and metals below iron in the E. M. P.series and of a metal selected from the group consisting of barium andmetals having not more than four electron orbits selected from groups I,II and III of the periodic system, and the reaction product ofphosphorus pentasulphide and degras reacted at a temperature to separatea, phosphorus and oxygen-containing residue.

8. Compounds of arsenic and of calcium, and the reaction product of asulphide of phosphorus and degras reacted at a temperature to separate aphosphorus and oxygen-containing residue.

9. Compounds of antimony and of barium, and the reaction product or asulphide oi phosphorus and degras reacted at a temperature to separate aphosphorus and oxygen-containing residue.

10. Compounds of chromium and of barium, and the reaction product of asulphide or phosphorus and degras reacted at a temperature to separate aphosphorus and oxygen-containing residue.

11. Compounds of a heavy metal selected from the group consisting ofchromium and metals below iron in the E. M. F. series and of a metalhaving not more than four electron orbits selected from groups LII andIII of the periodic system,

4 and the reaction product or a sulphide of phosphorus and anomen-containing wax.

12. The process for making a composition or matter suitable tor use as alubricant or as an addition agent to improve the characteristics oflubricating oi1,comprising reacting a sulphide of phosphorus with anoxygen-containing wax at a temperature to convert the phosphorus to aphosphorus and oxygen-containing compound which separates in a residueremoving said residue from the reaction product, and reacting saidproduct with compounds of a heavy metal selected from the groupconsisting of chromium and metals below iron in the E. M. F. series andor a. metal having not more than six electron orbits selected fromgroups I, II and m or the periodic system. to iorm the correspondingmetal compounds of said iirst reaction product.

13. The process for making a composition of matter suitable for use as alubricant or as an addition agent to improve the characteristics oflubricating 011. comprising reacting phosphorus pentasulphide with anoxygen-containing wax at a temperature to convert the phosphorus to anoxide, removing said residue from the reaction product, and reactingsaid product with compounds of a heavy metal selected irom the groupconsisting of chromium and metals below iron in the E. M. 1''. seriesand or a metal having not more than six electron orbits selected fromgroups I, II and III or the periodic system, to form the correspondingmetal compounds of said first reaction product.

14. The process for making a composition of matter suitable for use asa. lubricant or as an addition agent to improve the characteristics oflubricating oil, comprising reacting a sulphide of phos horus withdegras at a. temperature to convert the phosphorus to a phosphorus andoxygencontaining compound which separates in a residue removing saidresidue from the reaction product, and reacting said product withcompounds of a heavy metal selected from the group consisting ofchromium and metals below iron in the E. M. F. series and of a metalhaving not more than six electron orbits selected from groups I, II andIII of the periodic system, to form the corresponding metal compounds orsaid first reaction product.

15. The process for making a composition of matter suitable for use asa, lubricant or as an addition agent to improve the characteristics oflubricating oil, comprising reacting a sulphide of phosphorus withdegras at a temperature to convert the phosphorus to a phosphorus andoxygencontaining compound which separates in a residue removing saidresidue from the reaction product, and reacting said product withcompounds ot arsenic and of calcium to form arsenic and calciumcompounds of said first reaction product.

16. The process for making a composition of matter suitable for use as alubricant or as an addition agent to improve the characteristics oflubricating oil, comprising reacting a sulphide of phosphorus withdegras at a temperature to convert the phosphorus to a phosphorus andoxygencontaining compound which separates in a residue removing saidresidue from the reaction product, and reacting said product withcompounds of antimonv and of barium to form antimany and bariumcompounds of said first reaction product.

17. The process for making a composition oi matter suitable for use asa. lubricant or as an REFERENCES CITED The following references are ofrecord in the 15 file of this patent:

UNITED STATES PATENTS Number Name Date 2,237,096 Dearborn Apr. 1, 19412,331,923 Musselman Oct. 19, 1943 2,283,445 Reit! Nov. 18, 19412,257,751 Lincoln Oct. '7, 1941 2,211,306 Whittier Aug. 13, 19401,167,076 Jarlnan June 24, 1930 FOREIGN PATENTS Number Country Date521,656 Great Britain May 28, 1940 OTHER REFERENCES Handbook ofChemistry and Physics, Hodgman, 21st ad, page 695.

Certificate of Correction Patent No. 2,439,820.

April 20, 1948.

JOHN M. MUSSELMAN It is hereby certified that error appears in theoprinted specification of the above numbered patent requiringccorrectionas follows:

ted mm the group consisting of barium and metals; and that the word"metal insert se olumn 3, line 73, claim 11, after the said LettersPatent should e read with this correction therein that the same mayconform to the record of the case in the Patent Oflice.

Signed and sealed this 15th day of June, A. D. 1948.

THOMAS F. MURPHY,

Assistant Commissioner of Patents.

REFERENCES CITED The following references are of record in the 15 fileof this patent:

UNITED STATES PATENTS Number Name Date 2,237,096 Dearborn Apr. 1, 19412,331,923 Musselman Oct. 19, 1943 2,283,445 Reit! Nov. 18, 19412,257,751 Lincoln Oct. '7, 1941 2,211,306 Whittier Aug. 13, 19401,167,076 Jarlnan June 24, 1930 FOREIGN PATENTS Number Country Date521,656 Great Britain May 28, 1940 OTHER REFERENCES Handbook ofChemistry and Physics, Hodgman, 21st ad, page 695.

Certificate of Correction Patent No. 2,439,820.

April 20, 1948.

JOHN M. MUSSELMAN It is hereby certified that error appears in theoprinted specification of the above numbered patent requiringccorrectionas follows:

ted mm the group consisting of barium and metals; and that the word"metal insert se olumn 3, line 73, claim 11, after the said LettersPatent should e read with this correction therein that the same mayconform to the record of the case in the Patent Oflice.

Signed and sealed this 15th day of June, A. D. 1948.

THOMAS F. MURPHY,

Assistant Commissioner of Patents.

